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1、第6卷第2期食品安全质量检测学报Vol.6No.22015年2月JournalofFoodSafetyandQualityFeb.,2015液相色谱-串联质谱法测定保健品中L-羟脯氨酸含量*蔡伟江,陈晓霞(汤臣倍健股份有限公司,珠海519040)摘要:目的通过优化保健品中L-羟脯氨酸的测定条件,建立保健品中L-羟脯氨酸的液相色谱-串联质谱(LC-MS/MS)定量检测的分析方法。方法采用酸水解的方法处理L-羟脯氨酸,色谱柱(EC-C18,4.6mm×50mm,2.7μm),流动相为水相和乙腈按一定的梯度进行洗
2、脱,流速0.5mL/min,采用LC-MS/MS在正离子模式下检测,外标法定量。结果LC-MS/MS法在0.00284mg/mL~0.0284mg/mL范围内,L-羟脯氨酸的浓度和峰面积的线性2良好,相关系数R＞0.99,方法的检出限和定量限分别为1.42μg/g和4.7μg/g,放置24h内L-羟脯氨酸的稳定性良好,在不同添加水平下,方法的回收率范围为95.0%~98.8%,相对标准偏差为1.7%(n=9)。结论高效液相色谱-串联质谱法灵敏度高、准确、重现性好,适用于保健品中L-羟脯氨酸的含量测定。关键词
3、:L-羟脯氨酸;保健品;液相色谱-串联质谱法;含量测定DeterminationofL-hydroxyprolinecontentinhealthproductsbyhighperformanceliquidchromatography-tandemmassspectrometry*CAIWei-Jiang,CHENXiao-Xia(By-HealthCo.,Ltd.,Zhuhai519040,China)ABSTRACT:ObjectiveByoptimizingthedeterminationcondi
4、tionsofL-hydroxyprolineinhealthfoods,toestablishamethodforquantitativedeterminationofL-hydroxyprolinebyliquidchromatography-tandemmassspectrometry(LC-MS/MS).MethodsL-hydroxyprolinewasofacidhydrolysisandchromatographicanalysiswasperformedoncolumn(EC-C18,4.6
5、mm×50mm,2.7μm)elutedwithanacetonitrile-waterflowrateof0.5mL/min,whichwasdetectedbyLC-MS/MSinthepositiveionmodeandquantifiedbyexternalstandardmethod.ResultsThelinearrelationshipbetweenL-hydroxyprolineconcentrationandpeakareaweregood2within0.00284~0.0284mg/m
6、Lrange,R>0.99,thedetectionlimitandthelimitsofquantificationwere1.42μg/gand4.7μg/g,withagoodstabilityofL-hydroxyprolinewithin24h,andtherecoveryofdifferentaddinglevelswas95.0%~98.8%,andtherelativestandarddeviationwas1.7%(n=9).ConclusionHighperformanceliquidc
7、hromatography-tandemmassspectrometrymethodissensitive,accurate,reproducible,andapplicabletothedeterminationofL-hydroxyprolinecontentinhealthfoods.KEYWORDS:L-hydroxyproline;healthcareproducts;liquidchromatography-tandemmassspectrometry;contentdetermination*
8、通讯作者:蔡伟江,中药师,主要研究方向为保健食品的质量检测。E-mail:714524253@qq.com*Correspondingauthor:CAIWei-Jiang,Herbalists,By-HealthCo.,Ltd.,Zhuhai519040,China.E-mail:714524253@qq.com668食品安全质量检测学报第6卷0984V,纯度:100%);乙腈(色谱纯,CNW);乙酸铵(色1引
